Hydrochloric Acid → 6-[(2-Aminoethyl)amino]nicotinonitrile dihydrochloride

HRID 444810

反応式

HRID 444810 の反応式
[C:1]([C:3]1[CH:4]=[CH:5][C:6]([NH:9][CH2:10][CH2:11][NH:12]C(=O)OC(C)(C)C)=[N:7][CH:8]=1)#[N:2].[ClH:20]>O1CCOCC1>[ClH:20].[ClH:20].[NH2:12][CH2:11][CH2:10][NH:9][C:6]1[CH:5]=[CH:4][C:3]([C:1]#[N:2])=[CH:8][N:7]=1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 47453716tert-Butyl (2-((5-cyanopyridin-2-yl)amino)ethyl)carbamate

生成物 1

HCID 669113296-[(2-Aminoethyl)amino]nicotinonitrile dihydrochloride

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

7.9 g (30 mmol) of tert-butyl {2-[(5-cyanopyridin-2-yl)amino]ethyl}carbamate (Example 1A) were dissolved in 100 ml of 4N hydrogen chloride in dioxane and the mixture was stirred for 30 min. The reaction mixture was concentrated to half of its original volume and the same amount of diethyl ether was added. The reaction mixture was stirred for 20 min and the product was filtered off and washed with diethyl ether. This gave 7 g (94% of theory) of the product as a solid.

後処理

  1. concentrationThe reaction mixture was concentrated to half of its original volume
  2. additionthe same amount of diethyl ether was added
  3. stirringThe reaction mixture was stirred for 20 min
  4. filtrationthe product was filtered off
  5. washwashed with diethyl ether

出典と根拠

ORDレコード
ord-43f92318cda642ed868838c8d8031caf
出典データセット
uspto-grants-2013_07
特許番号
US08476267B2

関連ノート

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